CN102944545A - Nano-gold surface-enhanced Raman active substrate with layered three-dimensional structure and method for preparing same - Google Patents
Nano-gold surface-enhanced Raman active substrate with layered three-dimensional structure and method for preparing same Download PDFInfo
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Abstract
A nano-gold surface-enhanced Raman active substrate with a layered three-dimensional structure and a method for preparing the same relate to the fields of the nanometer materials science, laser Raman and biochemical analysis and detection. The surface-enhanced Raman active substrate is composed of three layers in total: a gold film, a dielectric layer and a two-dimensional array of irregular nano-gold particles arranged orderly from the bottom upwards, wherein the size and shape of the nano-gold particles and the thickness of each layer are adjustable. The method for preparing the substrate provided by the invention is to deposit the layered three-dimensional structure on a commercial glass slide with gold and silicon dioxide as coating materials by the ion beam coating method without using any other method. The nano-gold surface-enhanced Raman active substrate with the layered three-dimensional structure solves the problems of poor signal, low sensitivity, complex preparation process, high cost and the like of the nano-gold surface-enhanced Raman active substrate prepared by the prior art, and can be used for analyzing and detecting low-content compounds.
Description
Technical field
The present invention relates to a kind of stratiform three-dimensional structure nm of gold surface reinforced Raman active substrate and preparation method thereof.
Background technology
Since nineteen twenty-seven was found Ramam effect, Raman spectroscopy was real-time because having, harmless, the characteristics of fast detecting, is widely used in fields such as physics, biology, chemistry, medical science.But because Raman scattering efficient is very low, weak output signal, common Raman spectroscopy is difficult to trace materials, unimolecule behavior (such as conformation change, mutually identification, interaction etc.) etc. is carried out Real-Time Monitoring.1974, the discoveries such as the Fleischaman Raman signal that Adsorption of Pyridine can be enhanced on the silver electrode rough surface, Surface enhanced raman spectroscopy that Here it is (Surface-enhanced Raman scattering is referred to as SERS).Because Surface enhanced raman spectroscopy can greatly be carried high molecular raman scattering cross section, therefore, the spectral technique of setting up based on Surface enhanced raman spectroscopy has sensitivity and the molecular fingerprint ability of superelevation, is widely applied in the research of the aspects such as trace analysis, Single Molecule Detection, nano material, chemical industry, environmental science, biomedicine and sensing.
Surface enhanced raman spectroscopy mainly depends on the architectural feature of substrate, as form, how much, size and shape etc.Theoretical research shows, because exciting of local surface plasma, in tip, tie point or the space of metal nanoparticle and coarse metal surface and strong electromagnetic field (being focus) can appear, the Raman signal that is adsorbed on the molecule of these positions will obtain the enhancing of 8-10 the order of magnitude.Therefore, in recent years, the researchist has the surface enhanced Raman scattering substrate of certain roughness to carry out a large amount of research at the preparation table mask, has developed the preparation method of many surface enhanced Raman scattering substrates.Up to the present, many surface enhanced Raman scattering substrates based on different metal (gold, silver, copper and a small amount of alkaline metal such as sodium, potassium and lithium etc.) have appearred, such as surface enhanced Raman scattering substrates such as coarse electrode surface, nano particle polymkeric substance (comprising nanosphere, flower, polyhedron, dendron and crescent etc.), nano-grain array, nanometer metallic films.Yet, the drawbacks limit such as complicated process of preparation, cost are high, the preparation area is little, sensitivity is low, homogeneity is poor the application of surface enhanced Raman scattering substrate in fields such as trace materials, Single Molecule Detection.Obtain corresponding continuously 3-D nano, structure silver surface such as the control reduction silver ion behind polyaniline film assembling golden nanometer particle of reporting among the patent CN101566571 and strengthen the raman scattering spectrum substrate, overcome the poor problem of signal homogeneity, improved sensitivity, but still have complicated process of preparation to a certain extent, the high in cost of production problem.Surface enhanced Raman scattering substrate such as the electron beam lithography preparation, can control at the nanometer scale shape and the position of each particle, prepare uniform surface enhanced Raman scattering substrate, but the particle gap that makes causes sensitivity low more than 20 nanometers, consuming time and expensive.
Summary of the invention
The object of the present invention is to provide a kind of stratiform three-dimensional structure nm of gold surface reinforced Raman active substrate and preparation method thereof, the surface enhanced Raman scattering substrate sensitivity that solves the prior art preparation is low, complicated process of preparation, cost is high and the signal homogeneity is poor problem.
The present invention is achieved like this, the substrate of stratiform three-dimensional structure nm of gold surface reinforced Raman active is characterized in that the substrate of stratiform three-dimensional structure nm of gold surface reinforced Raman active is comprised of golden film, deielectric-coating and two-dimensional nano gold grain array successively from bottom to top.
The thickness of described golden film is 100 nm.
The thickness of described deielectric-coating is 20-60nm, and material is silicon dioxide.
The particle diameter of nanogold particle is 5-70 nm in the described nano gold layer.
Described nanogold particle out-of-shape, gap mean value is less than 10 nm between particle.
The sedimentation time of described two-dimensional nano array of particles preparation process intermediate ion bundle is 1.0-2.5 min.
The purposes of described stratiform three-dimensional structure nm of gold surface reinforced Raman active substrate, for detection of the organic molecule in the solution, such as rhodamine 6G, concentration detects can reach 1.0 μ mol/L with the substrate of layered three-dimensional structure nm of gold surface reinforced Raman active.
The purposes of described stratiform three-dimensional structure nm of gold surface reinforced Raman active substrate, the method that detects for organic molecule in the solution is, with the substrate of stratiform three-dimensional structure nm of gold surface reinforced Raman active as the Raman detection substrate, insert in the organic molecule solution of 1.0 μ mol/L, dip and do Raman detection after taking-up is dried after 24 hours.
The preparation method of described stratiform three-dimensional structure nm of gold surface reinforced Raman active substrate, method comprises the following steps:
1. accurately control the thickness of golden film by the film thickness watch-dog that utilizes the ion beam deposition instrument, 5 * 10
– 6Under the pressure of holder, with the plated film speed of 0.7/s with golden plated film on microslide, obtain ground floor structure-golden film;
2. 5 * 10
– 6Under the pressure of holder, with the plated film speed of 0.7/s with the silicon dioxide plated film to the golden film of step 1), the plated film time is 5-10 minute, obtains golden film-deielectric-coating double-decker;
3. 5 * 10
– 6Under the pressure of holder, with the plated film speed of 0.7/s with golden plated film to golden film-deielectric-coating double-decker, the plated film time is 1.0-2.5 minute, formation has erose two-dimensional nano gold grain array, obtains signal homogeneous, highly sensitive stratiform three-dimensional structure nm of gold surface reinforced Raman active substrate.
Technique effect of the present invention is: the surface enhanced Raman scattering substrate that utilizes the present invention to prepare, and its spectral signal is strong, detection sensitivity is high and signal response is even, and the quick nondestructive that can be widely used in low concentration organic molecule and biomolecule detects.The preparation method of laminate three-dimensional structure nm of gold surface reinforced Raman active of the present invention substrate, technique Simple fast, relative low price can obtain the stratiform three-dimensional structure nm of gold surface reinforced Raman active substrate that large-area metal construction is even, Raman signal is strong.Among the present invention, only use the ion beam deposition instrument, need not any other external condition and technique, reduced preparation technology's cost, and in wider dynamic range, can obtain reliable, stable, uniform Surface enhanced raman spectroscopy signal.Test shows, the rhodamine 6G solution of 1.0 μ mol/L is immersed in the surface-enhanced Raman scattering activity substrate of the inventive method preparation, measure its Raman spectrum and be golden film 2000 times.
Description of drawings
Describe the present invention in detail below in conjunction with the drawings and specific embodiments:
Fig. 1 stratiform three-dimensional structure nm of gold surface reinforced Raman active underlying structure schematic diagram;
The front scan electron micrograph image of Fig. 2 stratiform three-dimensional structure nm of gold surface reinforced Raman active substrate, the plated film time of two-dimensional nano gold grain array is respectively: (a) 1.0 min, (b) 1.5 min, (c) 2.0 min;
The side scanning electron microscopy picture of Fig. 3 stratiform three-dimensional structure nm of gold surface reinforced Raman active substrate, the thickness of middle dielectric layer is 40 nm;
Fig. 4 stratiform three-dimensional structure nm of gold surface reinforced Raman active substrate intermediate medium layer thickness is 20,40 and 60 nm, the Raman spectrogram when the nanogold particle plated film time is 1.0 min;
Fig. 5 stratiform three-dimensional structure nm of gold surface reinforced Raman active substrate intermediate medium layer thickness is 20,40 and 60 nm, the Raman spectrogram when the nanogold particle plated film time is 1.5 min;
Fig. 6 stratiform three-dimensional structure nm of gold surface reinforced Raman active substrate intermediate medium layer thickness is 20,40 and during 60 nm, and the nanogold particle plated film time is the Raman spectrogram of 2.0 min;
When Fig. 7 stratiform three-dimensional structure nm of gold surface reinforced Raman active substrate (1) intermediate medium layer thickness is 40 nm, change the Raman spectrogram of nanogold particle array plated film time, the plated film time is respectively 1,1.5,2 and 2.5 min;
Fig. 8 dielectric layer is 40 nm, and the nanogold particle array plated film time is when being 1.5 min, the Raman spectrum of the Raman spectrum of stratiform three-dimensional structure nm of gold surface reinforced Raman active substrate and golden film (100 nm) surface reinforced Raman active substrate.
Embodiment
The present invention is described in further detail below in conjunction with drawings and Examples, should understand these embodiment and only be used for explanation the present invention and be not used in and limit the scope of the invention.
Embodiment 1:
As shown in Figure 1, the stratiform three-dimensional structure nm of gold surface reinforced Raman active substrate in the present embodiment is comprised of golden film (1), silica dioxide medium layer (2) and two-dimensional nano gold grain array (3) from bottom to top successively.The structural representation of present embodiment laminate three-dimensional structure nm of gold surface reinforced Raman active substrate preparation as shown in Figure 1.The substrate of present embodiment laminate three-dimensional structure nm of gold surface reinforced Raman active can be widely used in the analyzing and testing of low concentration organic molecule and biomolecule.
Embodiment 2:
Present embodiment adopts gold and two kinds of materials of silicon dioxide, and at first on microslide, adopting method deposition a layer thickness of ion beam deposition is the golden film of 100 nm; Secondly, adopting the method deposit thickness of ion beam deposition at this golden film substrate is the silica dioxide medium film of 40 nm; At last, adopt method Direct precipitation two-dimensional nano gold grain array on this golden film-deielectric-coating of ion beam deposition.Present embodiment and embodiment example 1 are different is that the mean grain size of nanogold particle in the substrate of stratiform three-dimensional structure nm of gold surface reinforced Raman active is 5-70 nm, and other parameter is identical with embodiment example 1.
In the present embodiment two-dimensional nano gold grain array (3) of the stratiform three-dimensional structure nm of gold surface reinforced Raman active substrate that obtains is carried out surface microscopic topographic and characterize, as shown in Figure 2.As seen from Figure 2, in the array of particles (3), being evenly distributed of irregular nanogold particle, particle diameter is distributed between the 5-70 nm.
Embodiment 3:
Present embodiment is different from specific embodiment 1 or 2 is that middle dielectric layer (2) thickness of stratiform three-dimensional structure nm of gold surface reinforced Raman active substrate is 20-60 nm, and other parameter is identical with embodiment example 1 or 2.
Side microscopic appearance with the three-dimensional structure of the stratiform three-dimensional structure nm of gold surface reinforced Raman active substrate that obtains in the present embodiment characterizes, as shown in Figure 3.As seen from Figure 3, this structure has obvious three-decker, and even thickness.
Embodiment 4:
Present embodiment prepares the method for specific embodiment 1 described stratiform three-dimensional structure nm of gold surface reinforced Raman active substrate, realizes by following steps: 1) accurately control the thickness of golden film by the film thickness watch-dog that utilizes the ion beam deposition instrument, 5 * 10
– 6Under the pressure of holder, with the plated film speed of 0.7/s with golden plated film on microslide, obtain ground floor structure-golden film; 2) 5 * 10
– 6Under the pressure of holder, with the plated film speed of 0.7/s with the silicon dioxide plated film to the golden film of step 1), the plated film time is 5-10 minute, obtains golden film-deielectric-coating double-decker; 3) 5 * 10
– 6Under the pressure of holder, with the plated film speed of 0.7/s with golden plated film to golden film-deielectric-coating double-decker, the plated film time is 1.0-2.5 minute, formation has erose nanogold particle two-dimensional array, obtains signal homogeneous, highly sensitive stratiform three-dimensional structure nm of gold surface reinforced Raman active substrate.
Preparation technology's Simple fast in the present embodiment, navigability are strong, can obtain the stratiform three-dimensional structure nm of gold surface reinforced Raman active substrate that large-area metal construction is even, Raman signal is strong.The formation of this three-decker all just utilizes the method for ion beam deposition to obtain, and need not any other external condition and technique, has reduced preparation technology's cost.
Embodiment 5:
Present embodiment is soaked the stratiform three-dimensional structure nm of gold surface reinforced Raman active substrate that obtains in above-described embodiment 4 after 24 hours and is taken out in the rhodamine 6G solution of 1.0 μ mol/L, with in high-purity argon gas, drying after the deionized water washing, then survey its Raman signal, the gained Raman spectrogram as shown in Figure 4.As seen from Figure 4, when the nanogold particle array plated film time was 1.5 min, when the intermediate medium layer thickness was 40 nm, the Raman signal that obtains was a lot of by force.
Embodiment 6:
Present embodiment is soaked the stratiform three-dimensional structure nm of gold surface reinforced Raman active substrate that obtains in above-described embodiment 4 after 24 hours and is taken out in the rhodamine 6G solution of 1.0 μ mol/L, with in high-purity argon gas, drying after the deionized water washing, then survey its Raman signal, the gained Raman spectrogram as shown in Figure 5.As seen from Figure 5, when the nanogold particle array plated film time was 1.5 min, when the intermediate medium layer thickness was 40 nm, the Raman signal that obtains was a lot of by force.
Embodiment 7:
Present embodiment is soaked the stratiform three-dimensional structure nm of gold surface reinforced Raman active substrate that obtains in above-described embodiment 4 after 24 hours and is taken out in the rhodamine 6G solution of 1.0 μ mol/L, with in high-purity argon gas, drying after the deionized water washing, then survey its Raman signal, the gained Raman spectrogram as shown in Figure 6.As seen from Figure 6, when the nanogold particle array plated film time was 1.5 min, when the intermediate medium layer thickness was 40 nm, the Raman signal that obtains was a lot of by force.
In the time of can determining that by embodiment 5-7 the intermediate medium layer thickness is 40nm, the Raman signal of stratiform three-dimensional structure nm of gold surface reinforced Raman active substrate is the strongest.
Embodiment 8:
Present embodiment is with comprehensive above-described embodiment 4 and 5-7, preparation intermediate medium layer thickness is the stratiform three-dimensional structure nm of gold surface reinforced Raman active substrate of 40 nm, in the rhodamine 6G solution of 1.0 μ mol/L, soak after 24 hours and take out, with in high-purity argon gas, drying after the deionized water washing, then survey its Raman signal, the gained Raman spectrogram, as shown in Figure 7.As seen from Figure 7, when middle dielectric layer thickness is 40 nm, the plated film time of nanogold particle array, the Raman signal that obtains was the strongest when being 1.5 min.
Embodiment 9:
Present embodiment is with comprehensive above-described embodiment 4 and 5-7, preparation intermediate medium layer thickness is 40 nm, two-dimensional nano gold grain plated film time to be the stratiform three-dimensional structure nm of gold surface reinforced Raman active substrate of 1.5 min and the golden film in above-described embodiment 2, in the rhodamine 6G solution of 1.0 μ mol/L, soak after 24 hours and take out, with in high-purity argon gas, drying after the deionized water washing, then survey its Raman signal, gained Raman spectrum distribution plan as shown in Figure 8.As seen from Figure 8, to be positioned at 1650 cm
-1The Raman peaks at place as a comparison, the Raman signal of stratiform three-dimensional structure nm of gold surface reinforced Raman active substrate is 2000 times of golden film activity substrate Raman signal, can be used for the analyzing and testing to low concentration organic molecule, biomolecule.
Claims (9)
1. stratiform three-dimensional structure nm of gold surface reinforced Raman active substrate is characterized in that the substrate of stratiform three-dimensional structure nm of gold surface reinforced Raman active is comprised of golden film (1), deielectric-coating (2) and two-dimensional nano gold grain array (3) successively from bottom to top.
2. stratiform three-dimensional structure nm of gold surface reinforced Raman active according to claim 1 substrate, the thickness that it is characterized in that golden film (1) is 100 nm.
3. stratiform three-dimensional structure nm of gold surface reinforced Raman active according to claim 1 substrate, the thickness that it is characterized in that deielectric-coating (2) is 20-60nm, material is silicon dioxide.
4. stratiform three-dimensional structure nm of gold surface reinforced Raman active according to claim 1 substrate is characterized in that the particle diameter of nanogold particle in the nano gold layer (3) is 5-70 nm.
5. stratiform three-dimensional structure nm of gold surface reinforced Raman active according to claim 4 substrate, it is characterized in that: the nanogold particle out-of-shape, gap mean value is less than 10 nm between particle.
6. stratiform three-dimensional structure nm of gold surface reinforced Raman active according to claim 4 substrate is characterized in that: the sedimentation time of two-dimensional nano array of particles preparation process intermediate ion bundle is 1.0-2.5 min.
7. the purposes of a stratiform three-dimensional structure nm of gold surface reinforced Raman active as claimed in claim 1 substrate, it is characterized in that: with the substrate of layered three-dimensional structure nm of gold surface reinforced Raman active for detection of the organic molecule in the solution, such as rhodamine 6G, concentration detects can reach 1.0 μ mol/L.
8. the purposes of stratiform three-dimensional structure nm of gold surface reinforced Raman active according to claim 7 substrate, it is characterized in that: the method that detects for organic molecule in the solution is, with the substrate of stratiform three-dimensional structure nm of gold surface reinforced Raman active as the Raman detection substrate, insert in the organic molecule solution of 1.0 μ mol/L, dip and do Raman detection after taking-up is dried after 24 hours.
9. the preparation method of a stratiform three-dimensional structure nm of gold surface reinforced Raman active claimed in claim 1 substrate is characterized in that described method comprises the following steps:
Accurately control the thickness of golden film by the film thickness watch-dog that utilizes the ion beam deposition instrument, 5 * 10
– 6Under the pressure of holder, with the plated film speed of 0.7/s with golden plated film on microslide, obtain ground floor structure-golden film;
5 * 10
– 6Under the pressure of holder, with the plated film speed of 0.7/s with the silicon dioxide plated film to the golden film of step 1), the plated film time is 5-10 minute, obtains golden film-deielectric-coating double-decker;
5 * 10
– 6Under the pressure of holder, with the plated film speed of 0.7/s with golden plated film to golden film-deielectric-coating double-decker, the plated film time is 1.0-2.5 minute, formation has erose two-dimensional nano gold grain array, obtains signal homogeneous, highly sensitive stratiform three-dimensional structure nm of gold surface reinforced Raman active substrate.
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